CN114314646B - Energy-saving wet-process yellow lead preparation process - Google Patents
Energy-saving wet-process yellow lead preparation process Download PDFInfo
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- CN114314646B CN114314646B CN202111501426.1A CN202111501426A CN114314646B CN 114314646 B CN114314646 B CN 114314646B CN 202111501426 A CN202111501426 A CN 202111501426A CN 114314646 B CN114314646 B CN 114314646B
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 129
- 239000007788 liquid Substances 0.000 claims abstract description 93
- 230000001590 oxidative effect Effects 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 230000008021 deposition Effects 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000002344 surface layer Substances 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 92
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 38
- 239000001301 oxygen Substances 0.000 claims description 38
- 229910052760 oxygen Inorganic materials 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 239000011261 inert gas Substances 0.000 claims description 21
- 238000005868 electrolysis reaction Methods 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- 238000005273 aeration Methods 0.000 claims description 16
- 238000005485 electric heating Methods 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 9
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 230000003750 conditioning effect Effects 0.000 claims 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 8
- 229910001882 dioxygen Inorganic materials 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Physical Or Chemical Processes And Apparatus (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses an energy-saving wet-process yellow lead preparation process, which comprises the following steps: s1, heating and melting a solid lead raw material in a lead dissolving furnace to form lead liquid; s2, sending the lead liquid into a reaction kettle through a filter cylinder, keeping the temperature in the reaction kettle between 360 and 450 ℃, and stirring the lead liquid by using a stirring rod; s3, introducing oxidizing gas above the lead liquid in the reaction kettle, so that the oxidizing gas oxidizes lead steam volatilized from the surface layer of the lead liquid to form PbO; s4, the PbO particles grow up and fall onto the surface of the lead liquid, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition; s5, discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, carrying out solid-liquid separation to obtain solid powder, and drying the solid powder to obtain the PbO.
Description
Technical Field
The invention relates to the technical field of yellow lead preparation, in particular to an energy-saving wet-process yellow lead preparation process.
Background
At present, lead ingot is generally prepared by the procedures of melting, pulverizing, dedusting, calcining, packaging and the like in the production of yellow lead (PbO). It is known that Plumbum Preparatium belongs to toxic chemicals, lead smoke and lead dust can be generated in the production process, and if the collection effect is poor, the human health of operators can be directly injured, and meanwhile, the environment can be polluted; in addition, the melting and calcining procedures in the production process belong to high energy consumption procedures, so that the energy consumption is greatly increased, and the production cost of the product is increased.
Disclosure of Invention
The invention aims to provide an energy-saving wet-process yellow lead preparation process, which overcomes the defects of the prior art.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
an energy-saving wet-process yellow lead preparation process comprises the following steps:
s1, heating and melting a solid lead raw material in a lead dissolving furnace to form lead liquid;
s2, sending the lead liquid into a reaction kettle through a filter cylinder, keeping the temperature in the reaction kettle between 360 and 450 ℃, and stirring the lead liquid by using a stirring rod;
s3, introducing oxidizing gas above the lead liquid in the reaction kettle, so that the oxidizing gas oxidizes lead steam volatilized from the surface layer of the lead liquid to form PbO;
s4, the PbO particles grow up and fall onto the surface of the lead liquid, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition;
and S5, discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, carrying out solid-liquid separation to obtain solid powder, and drying the solid powder to obtain the PbO.
Preferably, the oxidizing gas is nitrogen containing 60-70wt% of oxygen.
Preferably, the oxidizing gas consists of the following gases in weight percent: 60-70% of oxygen, 0.2-0.5% of water vapor and the balance of nitrogen.
Preferably, the lower part of the lead liquid in the reaction kettle is also blown with inert gas, the density of the lead liquid in the reaction kettle can be reduced by the inert gas, the formed PbO is prevented from being deposited on the bottom of the reaction kettle, and the flow ratio of the inert gas to the oxidizing gas when entering the reaction kettle is 0.2-0.3:1.
Preferably, the inert gas is nitrogen or nitrogen containing 10-15wt% carbon dioxide.
Preferably, the lead liquid in the reaction kettle does not exceed two thirds of the volume of the reaction kettle.
Preferably, the oxygen in the oxidizing gas is derived from oxygen produced by electrolysis of water. The oxygen generated by electrolyzing water has high purity and convenient production, and the oxygen production amount can be regulated by controlling the current of the power supply.
Compared with the prior art, the invention has the following implementation effects:
1. according to the invention, the PbO powder is prepared by fully contacting lead vapor generated by lead liquid evaporation at high temperature with oxidizing gas, the powder particles are fine, and the powder particles can be discharged from the bottom of the reaction kettle, so that the problem of difficult preparation of the PbO of micro-nano particles is effectively solved, the prepared PbO is convenient to separate, and the working efficiency is improved;
2. the invention effectively improves the reaction rate through the catalytic conversion of water vapor by using the oxidizing gas containing moisture;
3. according to the invention, the carbon dioxide-containing gas is blown in from the lower part of the lead liquid, so that on one hand, the particle size of PbO is reduced, and meanwhile, the carbon dioxide and the water vapor promote the oxidation speed of lead vapor by oxygen, so that the production speed is improved, and on the other hand, the density of the lead liquid is effectively reduced, and the formed PbO particles can be quickly settled to the bottom of the reaction kettle;
4. on the one hand, the invention can effectively avoid the harm of lead fume and lead dust to human bodies and social environment, and simultaneously, the oxygen generated by electrolysis of water is used as a gas source of oxidation gas, so that the energy conservation and consumption reduction can be realized, the market competitiveness of the product is improved, and hydrogen byproducts and the income of enterprises can be increased.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Reference numerals illustrate: 1. a lead dissolving furnace; 11. a filter screen; 2. a communicating pipe; 3. a reaction kettle; 31. a stop valve; 32. an exhaust port; 33. an air inlet hole; 4. a motor; 41. a stirring rod; 42. stirring paddles; 5. an electric heating sleeve; 6. an aeration rod; 7. an air inlet pipe; 8. an electrolytic cell; 80. an electrolyte; 81. regulating an air pipe; 82. an oxygen duct; 83. a hydrogen gas guide pipe; 9. an adjustable DC power supply; 91. a negative plate; 92. a positive plate; 10. and (5) lead liquid.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements to be referred to must have a specific direction to construct and operate in a specific direction, and thus should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Example 1
As shown in fig. 1, the energy-saving wet-process yellow lead preparation device comprises a reaction kettle 3 and a lead dissolving furnace 1, wherein an electric heating sleeve 5 is arranged outside the reaction kettle 3, and the electric heating sleeve 5 enables lead liquid 10 in the reaction kettle 3 to be always in a liquid state; the lead dissolving furnace 1 is communicated with the lower part of the reaction kettle 3 through the communicating pipe 2, the high stability of lead liquid 10 in the reaction kettle 3 is guaranteed through the communicating vessel effect, the motor 4 is installed at the top of the reaction kettle 3, the stirring rod 41 inserted into the reaction kettle 3 is connected to the rotating shaft of the motor 4, the stirring paddle 42 is arranged at the bottom of the stirring rod 41, the stirring paddle 42 is arranged in the reaction kettle 3 below the communicating pipe 2, the lead dissolving furnace 1, the motor 4 and the electric heating sleeve 5 are electrically connected with an external power supply, the filter screen 11 is further arranged at the communicating pipe 2 in the lead dissolving furnace 1, and solid lead in the lead dissolving furnace 1 can be prevented from entering the reaction kettle 3.
An aeration rod 6 is further arranged in the reaction kettle 3 below the stirring paddle 42, the aeration rod 6 is connected with an external inert gas source, gas in the inert gas source is nitrogen, a discharge hole is further formed in the bottom of the reaction kettle 3 below the aeration rod 6, a discharge pipe is arranged on the discharge hole, a stop valve 31 is arranged on the discharge pipe, a plurality of air inlets 33 are formed in the periphery of the upper part of the reaction kettle 3, the plurality of air inlets 33 are connected with an air inlet pipe 7 arranged outside the reaction kettle 3, the air inlet pipe 7 is connected with an oxidizing gas source, the gas in the oxidizing gas source is formed by mixing 40wt% of adjusting gas and 60wt% of oxygen, the adjusting gas is nitrogen, the oxygen in the oxidizing gas source can reach 70wt% at most, the formed PbO particles are too large due to the excessive oxygen, the quality of products is influenced, and the flow of the inert gas source is one fifth of the oxidizing gas flow; the top of reation kettle 3 still is equipped with gas vent 32, oxygen is made by electrolytic device, electrolytic device includes adjustable DC power supply 9, electrolysis trough 8 and the electrolyte 80 in the electrolysis trough 8, electrolyte 80 is the aqueous solution of sodium hydroxide, the bottom of electrolysis trough 8 is equipped with positive plate 92 and negative plate 91, and positive plate 92 and negative plate 91 set up respectively in a bottom open-ended gas collecting hood, hydrogen gas guide 83 and oxygen gas guide 82 are installed respectively at the top of two gas collecting hoods, positive plate 92 and negative plate 91 are connected with adjustable power electricity respectively, adjust gas pipe 81 and oxygen gas guide 82 and be connected, make oxygen and adjusting gas mix get into intake pipe 7.
The process using the above apparatus: heating and melting solid lead raw materials in a lead dissolving furnace to form lead liquid; the lead liquid is fed into a 500L reaction kettle through a filter cylinder, the lead liquid in the reaction kettle is one half of the volume of the reaction kettle, the maximum lead liquid is not more than two thirds of the volume of the reaction kettle, nitrogen is blown into the lower part of the lead liquid in the reaction kettle, the flow rate of the nitrogen is 3L/min, the temperature in the reaction kettle is kept at 400 ℃, the lead liquid is stirred by using a stirring rod, and the filter cylinder can filter out particulate impurities;
then, oxidizing gas is introduced above the lead liquid in the reaction kettle, the flow rate of the oxidizing gas is 15L/min, and the oxidizing gas oxidizes lead vapor volatilized from the surface layer of the lead liquid to form PbO.
PbO particles formed in oxidizing gas above the lead liquid grow up and then fall onto the surface of the lead liquid under the action of gravity, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition; and then discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, carrying out solid-liquid separation to obtain solid powder, drying the solid powder, and removing residual lead to obtain the PbO, wherein the average production per hour of the PbO is 43.6kg, and the particle size of the obtained PbO is 360-435 nm.
Example 2
As shown in fig. 1, the energy-saving wet-process yellow lead preparation device comprises a reaction kettle 3 and a lead dissolving furnace 1, wherein an electric heating sleeve 5 is arranged outside the reaction kettle 3, and the electric heating sleeve 5 enables lead liquid 10 in the reaction kettle 3 to be always in a liquid state; the lead dissolving furnace 1 is communicated with the lower part of the reaction kettle 3 through the communicating pipe 2, the high stability of lead liquid 10 in the reaction kettle 3 is guaranteed through the communicating vessel effect, the motor 4 is installed at the top of the reaction kettle 3, the stirring rod 41 inserted into the reaction kettle 3 is connected to the rotating shaft of the motor 4, the stirring paddle 42 is arranged at the bottom of the stirring rod 41, the stirring paddle 42 is arranged in the reaction kettle 3 below the communicating pipe 2, the lead dissolving furnace 1, the motor 4 and the electric heating sleeve 5 are electrically connected with an external power supply, the filter screen 11 is further arranged at the communicating pipe 2 in the lead dissolving furnace 1, and solid lead in the lead dissolving furnace 1 can be prevented from entering the reaction kettle 3.
An aeration rod 6 is further arranged in the reaction kettle 3 below the stirring paddle 42, the aeration rod 6 is connected with an external inert gas source, the gas in the inert gas source is nitrogen containing 10wt% of carbon dioxide, a discharge port is further arranged at the bottom of the reaction kettle 3 below the aeration rod 6, a discharge pipe is arranged on the discharge port, a stop valve 31 is arranged on the discharge pipe, a plurality of air inlets 33 are arranged on the periphery of the upper part of the reaction kettle 3, the plurality of air inlets 33 are connected with an air inlet pipe 7 arranged outside the reaction kettle 3, the air inlet pipe 7 is connected with an oxidizing gas source, the gas in the oxidizing gas source is formed by mixing 40wt% of regulating gas with 60wt% of oxygen, the regulating gas is nitrogen, the oxygen in the oxidizing gas source can reach 70wt% at most, the formed PbO particles are overlarge due to the excessive oxygen, the quality of products is influenced, and the flow of the inert gas source is one fifth of the oxidizing gas flow; the top of reation kettle 3 still is equipped with gas vent 32, oxygen is made by electrolytic device, electrolytic device includes adjustable DC power supply 9, electrolysis trough 8 and the electrolyte 80 in the electrolysis trough 8, electrolyte 80 is the aqueous solution of sodium hydroxide, the bottom of electrolysis trough 8 is equipped with positive plate 92 and negative plate 91, and positive plate 92 and negative plate 91 set up respectively in a bottom open-ended gas collecting hood, hydrogen gas guide 83 and oxygen gas guide 82 are installed respectively at the top of two gas collecting hoods, positive plate 92 and negative plate 91 are connected with adjustable power electricity respectively, adjust gas pipe 81 and oxygen gas guide 82 and be connected, make oxygen and adjusting gas mix get into intake pipe 7.
The process using the above apparatus: heating and melting solid lead raw materials in a lead dissolving furnace to form lead liquid; the lead liquid is fed into a 500L reaction kettle through a filter cylinder, the lead liquid in the reaction kettle is one half of the volume of the reaction kettle, nitrogen containing 10wt% of carbon dioxide is blown into the lower part of the lead liquid in the reaction kettle, the gas flow is 5L/min, the temperature in the reaction kettle is kept at 450 ℃, and the lead liquid is stirred by using a stirring rod, so that the filter cylinder can filter out particulate impurities;
then, oxidizing gas is introduced above the lead liquid in the reaction kettle, the flow rate of the oxidizing gas is 15L/min, and the oxidizing gas oxidizes lead vapor volatilized from the surface layer of the lead liquid to form PbO.
PbO particles formed in oxidizing gas above the lead liquid grow up and then fall onto the surface of the lead liquid under the action of gravity, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition; and then discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, carrying out solid-liquid separation to obtain solid powder, drying the solid powder, and removing residual lead to obtain the PbO, wherein the average production per hour of the PbO is 41.3kg, and the particle size of the obtained PbO is 325-384 nm.
Example 3
As shown in fig. 1, the energy-saving wet-process yellow lead preparation device comprises a reaction kettle 3 and a lead dissolving furnace 1, wherein an electric heating sleeve 5 is arranged outside the reaction kettle 3, and the electric heating sleeve 5 enables lead liquid 10 in the reaction kettle 3 to be always in a liquid state; the lead dissolving furnace 1 is communicated with the lower part of the reaction kettle 3 through the communicating pipe 2, the high stability of lead liquid 10 in the reaction kettle 3 is guaranteed through the communicating vessel effect, the motor 4 is installed at the top of the reaction kettle 3, the stirring rod 41 inserted into the reaction kettle 3 is connected to the rotating shaft of the motor 4, the stirring paddle 42 is arranged at the bottom of the stirring rod 41, the stirring paddle 42 is arranged in the reaction kettle 3 below the communicating pipe 2, the lead dissolving furnace 1, the motor 4 and the electric heating sleeve 5 are electrically connected with an external power supply, the filter screen 11 is further arranged at the communicating pipe 2 in the lead dissolving furnace 1, and solid lead in the lead dissolving furnace 1 can be prevented from entering the reaction kettle 3.
An aeration rod 6 is further arranged in the reaction kettle 3 below the stirring paddle 42, the aeration rod 6 is connected with an external inert gas source, gas in the inert gas source is nitrogen, a discharge hole is further formed in the bottom of the reaction kettle 3 below the aeration rod 6, a discharge pipe is arranged on the discharge hole, a stop valve 31 is arranged on the discharge pipe, a plurality of air inlets 33 are formed in the periphery of the upper part of the reaction kettle 3, the plurality of air inlets 33 are connected with an air inlet pipe 7 arranged outside the reaction kettle 3, the air inlet pipe 7 is connected with an oxidizing gas source, the gas in the oxidizing gas source is formed by mixing 30wt% of adjusting gas and 70wt% of oxygen, the adjusting gas consists of nitrogen and water vapor, the mass ratio of the nitrogen to the water vapor is 39.8:0.2, the formed PbO particles are excessively large due to excessive oxygen, the quality of products is influenced, and the flow of the inert gas source is one fifth of the oxidizing gas flow; the top of reation kettle 3 still is equipped with gas vent 32, oxygen is made by electrolytic device, electrolytic device includes adjustable DC power supply 9, electrolysis trough 8 and the electrolyte 80 in the electrolysis trough 8, electrolyte 80 is the aqueous solution of sodium hydroxide, the bottom of electrolysis trough 8 is equipped with positive plate 92 and negative plate 91, and positive plate 92 and negative plate 91 set up respectively in a bottom open-ended gas collecting hood, hydrogen gas guide 83 and oxygen gas guide 82 are installed respectively at the top of two gas collecting hoods, positive plate 92 and negative plate 91 are connected with adjustable power electricity respectively, adjust gas pipe 81 and oxygen gas guide 82 and be connected, make oxygen and adjusting gas mix get into intake pipe 7.
The process using the above apparatus: heating and melting solid lead raw materials in a lead dissolving furnace to form lead liquid; the lead liquid is fed into a 500L reaction kettle through a filter cylinder, the lead liquid in the reaction kettle is one half of the volume of the reaction kettle, nitrogen is blown into the lower part of the lead liquid in the reaction kettle, the flow rate of the nitrogen is 5L/min, the temperature in the reaction kettle is kept at 380 ℃, the lead liquid is stirred by using a stirring rod, and the filter cylinder can filter out particulate impurities;
then, oxidizing gas is introduced above the lead liquid in the reaction kettle, the flow rate of the oxidizing gas is 15L/min, and the oxidizing gas oxidizes lead vapor volatilized from the surface layer of the lead liquid to form PbO.
PbO particles formed in oxidizing gas above the lead liquid grow up and then fall onto the surface of the lead liquid under the action of gravity, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition; and then discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, carrying out solid-liquid separation to obtain solid powder, drying the solid powder, and removing residual lead to obtain the PbO, wherein the average production per hour of the PbO is 48.2kg, and the particle size of the obtained PbO is 430-510 nm.
Example 4
As shown in fig. 1, the energy-saving wet-process yellow lead preparation device comprises a reaction kettle 3 and a lead dissolving furnace 1, wherein an electric heating sleeve 5 is arranged outside the reaction kettle 3, and the electric heating sleeve 5 enables lead liquid 10 in the reaction kettle 3 to be always in a liquid state; the lead dissolving furnace 1 is communicated with the lower part of the reaction kettle 3 through the communicating pipe 2, the high stability of lead liquid 10 in the reaction kettle 3 is guaranteed through the communicating vessel effect, the motor 4 is installed at the top of the reaction kettle 3, the stirring rod 41 inserted into the reaction kettle 3 is connected to the rotating shaft of the motor 4, the stirring paddle 42 is arranged at the bottom of the stirring rod 41, the stirring paddle 42 is arranged in the reaction kettle 3 below the communicating pipe 2, the lead dissolving furnace 1, the motor 4 and the electric heating sleeve 5 are electrically connected with an external power supply, the filter screen 11 is further arranged at the communicating pipe 2 in the lead dissolving furnace 1, and solid lead in the lead dissolving furnace 1 can be prevented from entering the reaction kettle 3.
An aeration rod 6 is further arranged in the reaction kettle 3 below the stirring paddle 42, the aeration rod 6 is connected with an external inert gas source, gas in the inert gas source is nitrogen containing 15wt% of carbon dioxide, a discharge port is further arranged at the bottom of the reaction kettle 3 below the aeration rod 6, a discharge pipe is arranged on the discharge port, a stop valve 31 is arranged on the discharge pipe, a plurality of air inlets 33 are arranged on the periphery of the upper part of the reaction kettle 3, the plurality of air inlets 33 are connected with an air inlet pipe 7 arranged outside the reaction kettle 3, the air inlet pipe 7 is connected with an oxidizing gas source, the gas in the oxidizing gas source is formed by mixing 30wt% of regulating gas and 70wt% of oxygen, the regulating gas consists of nitrogen and water vapor, the mass ratio of the nitrogen to the water vapor is 39.5:0.5, the formed PbO particles are excessively large due to excessive oxygen, the quality of products is influenced, and the flow of the inert gas source is one fifth of the oxidizing gas flow; the top of reation kettle 3 still is equipped with gas vent 32, oxygen is made by electrolytic device, electrolytic device includes adjustable DC power supply 9, electrolysis trough 8 and the electrolyte 80 in the electrolysis trough 8, electrolyte 80 is the aqueous solution of sodium hydroxide, the bottom of electrolysis trough 8 is equipped with positive plate 92 and negative plate 91, and positive plate 92 and negative plate 91 set up respectively in a bottom open-ended gas collecting hood, hydrogen gas guide 83 and oxygen gas guide 82 are installed respectively at the top of two gas collecting hoods, positive plate 92 and negative plate 91 are connected with adjustable power electricity respectively, adjust gas pipe 81 and oxygen gas guide 82 and be connected, make oxygen and adjusting gas mix get into intake pipe 7.
The process using the above apparatus: heating and melting solid lead raw materials in a lead dissolving furnace to form lead liquid; the lead liquid is fed into a 500L reaction kettle through a filter cylinder, the lead liquid in the reaction kettle is one half of the volume of the reaction kettle, nitrogen containing 15wt% of carbon dioxide is blown into the lower part of the lead liquid in the reaction kettle, the gas flow is 5L/min, the temperature in the reaction kettle is kept at 360 ℃, and the lead liquid is stirred by using a stirring rod, so that the filter cylinder can filter out particulate impurities;
then, oxidizing gas is introduced above the lead liquid in the reaction kettle, the flow rate of the oxidizing gas is 15L/min, and the oxidizing gas oxidizes lead vapor volatilized from the surface layer of the lead liquid to form PbO.
PbO particles formed in oxidizing gas above the lead liquid grow up and then fall onto the surface of the lead liquid under the action of gravity, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition; and then discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, carrying out solid-liquid separation to obtain solid powder, drying the solid powder, and removing residual lead to obtain the PbO, wherein the average production per hour of the PbO is 52.5kg, and the particle size of the obtained PbO is 310-350 nm.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. An energy-saving wet-process yellow lead preparation process is characterized by comprising the following steps:
s1, heating and melting a solid lead raw material in a lead dissolving furnace to form lead liquid;
s2, sending the lead liquid into a reaction kettle through a filter cylinder, keeping the temperature in the reaction kettle between 360 and 450 ℃, and stirring the lead liquid by using a stirring rod;
s3, introducing oxidizing gas above the lead liquid in the reaction kettle, so that the oxidizing gas oxidizes lead steam volatilized from the surface layer of the lead liquid to form PbO;
s4, the PbO particles grow up and fall onto the surface of the lead liquid, and the PbO particles reach the bottom of the reaction kettle after stirring and deposition;
s5, discharging the mixture of the lead liquid and the PbO from the bottom of the reaction kettle, performing solid-liquid separation to obtain solid powder, and drying the solid powder to obtain the PbO;
the energy-saving wet-process yellow lead is prepared by the following equipment and comprises a reaction kettle (3) and a lead dissolving furnace (1), wherein an electric heating sleeve (5) is arranged outside the reaction kettle (3), and the electric heating sleeve (5) enables lead liquid (10) in the reaction kettle (3) to be always in a liquid state; the lead dissolving furnace (1) is communicated with the lower part of the reaction kettle (3) through a communicating pipe (2), the high stability of lead liquid (10) in the reaction kettle (3) is ensured through a communicating vessel effect, a motor (4) is installed at the top of the reaction kettle (3), a stirring rod (41) inserted into the reaction kettle (3) is connected to a rotating shaft of the motor (4), a stirring paddle (42) is arranged at the bottom of the stirring rod (41), the stirring paddle (42) is arranged in the reaction kettle (3) below the communicating pipe (2), the lead dissolving furnace (1), the motor (4) and an electric heating sleeve (5) are electrically connected with an external power supply, and a filter screen (11) is further arranged at the communicating pipe (2) in the lead dissolving furnace (1) to prevent solid lead in the lead dissolving furnace (1) from entering the reaction kettle (3);
an aeration rod (6) is further installed in the reaction kettle (3) below the stirring paddle (42), the aeration rod (6) is connected with an external inert gas source, a discharge port is further formed in the bottom of the reaction kettle (3) below the aeration rod (6), a discharge pipe is installed on the discharge port, a stop valve (31) is installed on the discharge pipe, a plurality of air inlets (33) are formed in the periphery of the upper portion of the reaction kettle (3), the plurality of air inlets (33) are connected with an air inlet pipe (7) arranged outside the reaction kettle (3), the air inlet pipe (7) is connected with an oxidizing gas source, the top of the reaction kettle (3) is further provided with an exhaust port (32), oxygen is made of an electrolysis device, the electrolysis device comprises an adjustable direct current power supply (9), an electrolysis tank (8) and an electrolyte (80) in the electrolysis tank (8), the electrolyte (80) is an aqueous solution of sodium hydroxide, a positive plate (92) and a negative plate (91) are respectively arranged at the bottom of the electrolysis tank (8), the positive plate (92) and the negative plate (91) are respectively arranged in an air collecting hood with an opening at the bottom, an air guide pipe (83) and an oxygen guide pipe (82) are respectively arranged at the top of the two air collecting hoods, the oxygen guide pipe (82) and the oxygen guide pipe (82) are respectively connected with the oxygen guide pipe (81), oxygen and conditioning gas are mixed into the inlet pipe (7).
2. The process for preparing energy-saving wet-process yellow lead according to claim 1, wherein the oxidizing gas is air containing 60-70wt% of oxygen or is formed by mixing 40wt% of adjusting gas with 60-70wt% of oxygen, and the adjusting gas is nitrogen.
3. The energy-saving wet-process yellow lead preparation process according to claim 1, wherein the oxidizing gas consists of the following gases in percentage by weight: 60-70% of oxygen, 0.2-0.5% of water vapor and the balance of nitrogen.
4. An energy-saving wet-process yellow lead preparation process according to claim 3 and wherein the oxygen in the oxidizing gas is derived from oxygen generated by electrolysis of water.
5. The energy-saving wet-process yellow lead preparation process according to claim 1, wherein inert gas is blown into the lower part of the lead liquid in the reaction kettle, and the flow ratio of the inert gas to the oxidizing gas when the inert gas and the oxidizing gas enter the reaction kettle is 0.2-0.3:1.
6. The energy-saving wet process yellow lead preparation process according to claim 5, wherein the inert gas is nitrogen or nitrogen containing 10-15wt% of carbon dioxide.
7. The energy-saving wet-process yellow lead preparation process according to claim 1, wherein the lead liquid in the reaction kettle is not more than two thirds of the volume of the reaction kettle.
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